CN102181753B - Silicon and silicon carbide hybrid enhanced aluminum-base composite material and preparation method thereof - Google Patents

Silicon and silicon carbide hybrid enhanced aluminum-base composite material and preparation method thereof Download PDF

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Publication number
CN102181753B
CN102181753B CN 201110062275 CN201110062275A CN102181753B CN 102181753 B CN102181753 B CN 102181753B CN 201110062275 CN201110062275 CN 201110062275 CN 201110062275 A CN201110062275 A CN 201110062275A CN 102181753 B CN102181753 B CN 102181753B
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silicon
silicon carbide
powder
carbide
fine powder
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CN102181753A (en
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马俊立
杨军
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Zhen'an minko Electronic Materials Co. Ltd.
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Mingke Microelectronic Material Co Ltd Xi'an City
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Abstract

The invention relates to a silicon and silicon carbide hybrid enhanced aluminum-base composite material and a preparation method thereof, which overcome the shortcomings of the traditional single aluminum-silicon composite material or aluminum/silicon carbide composite material in performance. The silicon and silicon carbide hybrid enhanced aluminum-base composite material has the advantages of adjustable volume percent of the silicon or the silicon carbide within a certain range, low preparation cost and convenient process. In a technical scheme adopted by the invention, the composite material comprises the following ingredients in percentage by volume: 0-50% of coarse silicon carbide powder, 10-20% of fine silicon carbide powder, 5-10% of micro silicon carbide powder, 10-20% of fine silicon powder, 5-40% of micro silicon powder, 8-57% of metal aluminum element, 1.9-2.7% of metal silicon element and 0.1-0.3% of metal magnesium element; and the particle sizes of the coarse silicon carbide powder, the fine silicon carbide powder, the micro silicon carbide powder, the fine silicon powder and the micro silicon powder are respectively 120-210 microns, 30-63 microns, 6-12 microns, 30-50 microns and 6-12 microns.

Description

A kind of silicon and silicon carbide mix aluminum matrix composite of enhancing and preparation method thereof
One, technical field:
The present invention relates to a kind of metal-base composites, especially relate to a kind of carbide composite material with ultrahigh volume fraction and preparation method thereof.
Two, background technology:
In the background technology, Al-Si composites and aluminum silicon carbide composite material respectively have characteristics, the former has the advantages such as thermal expansivity is low, density is low, easy processing, easy coating, easy welding, the latter has the advantages such as thermal conductivity height, intensity is high, Young's modulus is high, wear resistance is good, therefore the characteristics with both combine, and can prepare the silicon of excellent combination property and the aluminum matrix composite that silicon carbide mixes enhancing.
Three, summary of the invention:
The present invention is in order to solve the weak point in the above-mentioned background technology, provide a kind of silicon and silicon carbide to mix aluminum matrix composite of enhancing and preparation method thereof, it has overcome existing single Al-Si composites or aluminum silicon carbide composite material in the deficiency of aspect of performance separately, the volume fraction of silicon or silicon carbide can be regulated within the specific limits, preparation cost is low, and technique is convenient, can realize complicated shape and large-sized near-net-shape, over-all properties can be regulated arbitrarily, and reliability is high.
For achieving the above object, the technical solution used in the present invention is:
A kind of silicon and silicon carbide mix the aluminum matrix composite of enhancing, it is characterized in that: described matrix material by volume per-cent is comprised of silicon carbide meal 0~50%, carbide fine powder 10~20%, silicon carbide micro-powder 5~10%, silica fine powder 10~20%, silicon powder 5~40%, metallic aluminium element 8~57%, Pure Silicon Metal element 1.9~2.7% and MAGNESIUM METAL element 0.1~0.3%; The particle diameter of described silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder is respectively 120~210 μ m, 30~63 μ m, 6~12 μ m, 30~50 μ m and 6~12 μ m.
Above-mentioned matrix material by volume per-cent is comprised of silicon carbide meal 46~48%, carbide fine powder 21~22%, silicon carbide micro-powder 6~8%, silica fine powder 15~18%, silicon powder 8~10%, metallic aluminium element 18~22%, Pure Silicon Metal element 1.9~2.7% and MAGNESIUM METAL element 0.1~0.3%; The particle diameter of described silicon carbide meal, carbide fine powder and silicon powder is respectively 120~210 μ m, 30~63 μ m and 6~12 μ m.
A kind of silicon and silicon carbide mix the preparation method of the aluminum matrix composite of enhancing, it is characterized in that may further comprise the steps:
Silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder packed into mix in the mixer, add again additive at the LPIM forming under the pressure; Be coated with shell with water glass and aluminum oxide powder at surface of shaped parts, drying, de-waxing and sintering are made and are with chlamydate silicon and silicon carbide hybrid preforms; Under vacuum and gaseous tension, aluminum alloy melt is impregnated in silicon and the silicon carbide hybrid preforms, solidify rear removal shell, form silicon and the silicon carbide hybrid reinforced aluminum-matrix composite material of the near-net-shape of complicated shape, the volume fraction sum of its silicon and silicon carbide is: 40%~80%.
The volume percent that above-mentioned additive accounts for raw material is paraffin 9~27%, oleic acid 1~3%.
Above-mentioned de-waxing and sintering process are: 2 ℃/min of de-waxing temperature rise rate~3 ℃/min, 100 ℃~120 ℃ of binder burnout temperatures, soaking time 240 min, 3 ℃/min of sintering temperature rise rate~5 ℃/min, 1050~1100 ℃ of sintering of sintering temperature 2~4 hours, rate of cooling was 10 ℃/min~20 ℃/min.
Compared with prior art, the advantage and the effect that have of the present invention is as follows:
The characteristics that the present invention gives prominence to are that the volume fraction with silicon and silicon carbide is regulated arbitrarily between 40%~80%, so the thermal expansivity of matrix material, thermal conductivity, intensity, Young's modulus, density, processibility etc. can be regulated and control as required; Metallic aluminium, Pure Silicon Metal and MAGNESIUM METAL element can carry out reasonably combined, have improved the mechanical property of material.Adopted the prefabrication type with shell, and used pressure is no more than 3MPa, therefore realized the near-net-shape of complicated shape part.Owing to vacuumize with pressure impregnation is disposable and finish, material compactness is high, does not therefore need complicated follow-up densification processing.Because mixing the various performances of the aluminum matrix composite of enhancing, this silicon and silicon carbide can regulate on a large scale, and part can be realized near-net-shape, therefore can be widely used in the fields such as microelectronics, power electronic, microwave, photoelectron, aerospace, automobile, have good society and economic benefit.
Four, embodiment:
The present invention is the aluminum matrix composite that a kind of silicon and silicon carbide mix enhancing, and by volume per-cent is comprised of silicon carbide meal 0~50%, carbide fine powder 10~20%, silicon carbide micro-powder 5~10%, silica fine powder 10~20%, silicon powder 5~40%, metallic aluminium element 8~57%, Pure Silicon Metal element 1.9~2.7% and MAGNESIUM METAL element 0.1~0.3%; The particle diameter of described silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder is respectively 120~210 μ m, 30~63 μ m, 6~12 μ m, 30~50 μ m and 6~12 μ m.
The better a kind of technical scheme of the present invention is: by volume per-cent is comprised of silicon carbide meal 46~48%, carbide fine powder 21~22%, silicon carbide micro-powder 6~8%, silica fine powder 15~18%, silicon powder 8~10%, metallic aluminium element 18~22%, Pure Silicon Metal element 1.9~2.7% and MAGNESIUM METAL element 0.1~0.3%; The particle diameter of described silicon carbide meal, carbide fine powder and silicon powder is respectively 120~210 μ m, 30~63 μ m and 6~12 μ m.
Preparation method of the present invention may further comprise the steps:
With the silicon carbide meal,, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder pack into and mixed 12~15 hours in the mixer; Add additive at 3MPa LPIM forming under the pressure, to account for the mass ratio of raw material be paraffin 18~53% to institute's doping during LPIM, oleic acid 1~4% again; Be coated with the shell of 5 bed thickness with water glass and aluminum oxide powder at surface of shaped parts, and 50 ℃~70 ℃ dryings 6~8 hours; Subsequently formed body and shell are carried out de-waxing and sintering, de-waxing and sintering process are: 2 ℃/min of de-waxing temperature rise rate~3 ℃/min, 100 ℃~120 ℃ of binder burnout temperatures, soaking time 240 min, 3 ℃/min of sintering temperature rise rate~5 ℃/min, 1050~1100 ℃ of sintering of sintering temperature 2~4 hours, rate of cooling was 10 ℃/min~20 ℃/min; With above-mentioned make be with chlamydate silicon and silicon carbide hybrid preforms to put into the gas pressure infiltration stove to be preheating to 700 ℃, be evacuated down to 0.07MPa, under 2.0~3.0MPa gaseous tension, 800 ℃ aluminum alloy melt is impregnated in silicon and the silicon carbide hybrid preforms, solidify rear removal shell, form the silicon of near-net-shape and the aluminum matrix composite that silicon carbide mixes enhancing, the volume fraction sum of its silicon and silicon carbide is: 40%~80%.
Silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder all are high-purity powder.Metallic aluminium, Pure Silicon Metal and MAGNESIUM METAL all are the technical grade ingot metals.
Require as follows to raw-material chemical ingredients:
The title material index
Silicon carbide meal SiC 〉=99%
Carbide fine powder SiC 〉=99%
Silicon carbide micro-powder SiC 〉=99%
Silica fine powder SiC 〉=99%
Silicon powder SiC 〉=99%
Metallic aluminium Al 〉=99.7%
Pure Silicon Metal Si 〉=99.9%
MAGNESIUM METAL Mg 〉=99.9%
The material particle size scope: the particle diameter of silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder is respectively 120~210 μ m, 30~63 μ m, 6~12 μ m, 30~50 μ m and 6~12 μ m.
Embodiment 1:
With particle diameter be the carbide fine powder of 30~63 μ m and 6~12 μ m silicon powder by volume per-cent 25% and 25% pack into and mixed 12~15 hours in the mixer; Add additive at 3MPa LPIM forming under the pressure, to account for the mass ratio of raw material be paraffin 46% to institute's doping during LPIM, oleic acid 4% again; Be coated with the shell of 5 bed thickness with water glass and aluminum oxide powder at surface of shaped parts, and 50 ℃~70 ℃ dryings 6~8 hours; Subsequently formed body and shell are carried out de-waxing and sintering, de-waxing and sintering process are: 2 ℃/min of de-waxing temperature rise rate~3 ℃/min, 100 ℃~120 ℃ of binder burnout temperatures, soaking time 240 min, 3 ℃/min of sintering temperature rise rate~5 ℃/min, 1050~1100 ℃ of sintering of sintering temperature 2~4 hours, rate of cooling was 10 ℃/min~20 ℃/min; With above-mentioned make be with chlamydate silicon and silicon carbide hybrid preforms to put into the gas pressure infiltration stove to be preheating to 700 ℃, be evacuated down to 0.07MPa, under the 2.0MPa gaseous tension, 800 ℃ aluminum alloy melt is impregnated in silicon and the silicon carbide hybrid preforms, solidify rear removal shell, (matrix material is by volume by carbide fine powder 25% to form the silicon of near-net-shape and the aluminum matrix composite that silicon carbide mixes enhancing, silicon powder 25%, metallic aluminium element 47%, Pure Silicon Metal element 2.7% and MAGNESIUM METAL element 0.3% form), the volume fraction of its silicon and silicon carbide is: 25%, and the volume fraction sum is 50%.
Embodiment 2:
Be that the silicon powder of the carbide fine powder of 30~63 μ m and 6~12 μ m 40% and 20% is packed into and mixed 12~15 hours in the mixer by volume with particle diameter; Add additive at 3MPa LPIM forming under the pressure, to account for the mass ratio of raw material be paraffin 37% to institute's doping during LPIM, oleic acid 3% again; Be coated with the shell of 5 bed thickness with water glass and aluminum oxide powder at surface of shaped parts, and 50 ℃~70 ℃ dryings 6~8 hours; Subsequently formed body and shell are carried out de-waxing and sintering, de-waxing and sintering process are: 2 ℃/min of de-waxing temperature rise rate~3 ℃/min, 100 ℃~120 ℃ of binder burnout temperatures, soaking time 240 min, 3 ℃/min of sintering temperature rise rate~5 ℃/min, 1050~1100 ℃ of sintering of sintering temperature 2~4 hours, rate of cooling was 10 ℃/min~20 ℃/min; With above-mentioned make be with chlamydate silicon and silicon carbide hybrid preforms to put into the gas pressure infiltration stove to be preheating to 700 ℃, be evacuated down to 0.07MPa, under the 2.5MPa gaseous tension, 800 ℃ aluminum alloy melt is impregnated in silicon and the silicon carbide hybrid preforms, solidify rear removal shell, (matrix material is by volume by carbide fine powder 40% to form the silicon of near-net-shape and the aluminum matrix composite that silicon carbide mixes enhancing, silicon powder 20%, metallic aluminium element 37.5%, Pure Silicon Metal element 2.3% and MAGNESIUM METAL element 0.2% form), the volume fraction of its silicon and silicon carbide is respectively 20% and 40%, and the volume fraction sum is 60%.
Embodiment 3:
The silicon powder that with particle diameter is the carbide fine powder of silicon carbide meal, 30~63 μ m of 120~210 μ m and 6~12 μ m 45%, 23% and 12% is packed into and was mixed 12~15 hours in the mixer by volume; Add additive at 3MPa LPIM forming under the pressure, to account for the mass ratio of raw material be paraffin 17% to institute's doping during LPIM, oleic acid 2% again; Be coated with the shell of 5 bed thickness with water glass and aluminum oxide powder at surface of shaped parts, and 50 ℃~70 ℃ dryings 6~8 hours; Subsequently formed body and shell are carried out de-waxing and sintering, de-waxing and sintering process are: 2 ℃/min of de-waxing temperature rise rate~3 ℃/min, 100 ℃~120 ℃ of binder burnout temperatures, soaking time 240 min, 3 ℃/min of sintering temperature rise rate~5 ℃/min, 1050~1100 ℃ of sintering of sintering temperature 2~4 hours, rate of cooling was 10 ℃/min~20 ℃/min; With above-mentioned make be with chlamydate silicon and silicon carbide hybrid preforms to put into the gas pressure infiltration stove to be preheating to 700 ℃, be evacuated down to 0.07MPa, under the 3.0MPa gaseous tension, 800 ℃ aluminum alloy melt is impregnated in silicon and the silicon carbide hybrid preforms, solidify rear removal shell, (matrix material is by volume by silicon carbide meal 45% to form the silicon of near-net-shape and the aluminum matrix composite that silicon carbide mixes enhancing, carbide fine powder 23%, silicon powder 12%, metallic aluminium element 18%, Pure Silicon Metal element 1.9% and MAGNESIUM METAL element 0.1% form), the volume fraction of its silicon and silicon carbide is respectively 12% and 68%, and the volume fraction sum is 80%.
In sum, making method of the present invention is carried out in the steps below:
A, by the accurate weighing silicon carbide of ratio requirement meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder, mixed in the mixer of packing into 12~15 hours;
B, adopt the moulding of LPIM method, and be coated with the formation shell with water glass and aluminum oxide powder at surface of shaped parts, make porous silicon and silicon carbide hybrid preforms with shell behind drying, de-waxing and the sintering, sintering temperature is no more than 1100 ℃;
C, by proportioning metallic aluminium, Pure Silicon Metal and MAGNESIUM METAL are fused into alloy, under vacuum and pressure, make liquid alloy be impregnated into porous silicon and silicon carbide hybrid preforms, solidify the aluminum matrix composite that rear formation silicon and silicon carbide mix enhancing, pressure generally is not more than 3MPa;
D, according to drawing requirement, hybrid composite can come into operation after a small amount of processing.

Claims (2)

1. a silicon and silicon carbide mix the aluminum matrix composite of enhancing, and it is characterized in that: described matrix material by volume per-cent is comprised of silicon carbide meal 0~50%, carbide fine powder 10~20%, silicon carbide micro-powder 5~10%, silica fine powder 10~20%, silicon powder 5~40%, metallic aluminium element 8~57%, Pure Silicon Metal element 1.9~2.7% and MAGNESIUM METAL element 0.1~0.3%; The particle diameter of described silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder is respectively 120~210 μ m, 30~63 μ m, 6~12 μ m, 30~50 μ m and 6~12 μ m.
2. a kind of silicon according to claim 1 and silicon carbide mix the preparation method of the aluminum matrix composite of enhancing, it is characterized in that may further comprise the steps:
Silicon carbide meal, carbide fine powder, silicon carbide micro-powder, silica fine powder and silicon powder packed into mix in the mixer, add again additive at the LPIM forming under the pressure; Be coated with shell with water glass and aluminum oxide powder at surface of shaped parts, drying, de-waxing and sintering are made and are with chlamydate silicon and silicon carbide hybrid preforms; Under vacuum and gaseous tension, aluminum alloy melt is impregnated in silicon and the silicon carbide hybrid preforms, solidify rear removal shell, form silicon and the silicon carbide hybrid reinforced aluminum-matrix composite material of the near-net-shape of complicated shape, the volume fraction sum of its silicon and silicon carbide is: 40%~80%;
The volume percent that described additive accounts for raw material is paraffin 9~27%, oleic acid 1~3%;
De-waxing and sintering process are: 2 ℃/min of de-waxing temperature rise rate~3 ℃/min, 100 ℃~120 ℃ of binder burnout temperatures, soaking time 240 min, 3 ℃/min of sintering temperature rise rate~5 ℃/min, 1050~1100 ℃ of sintering of sintering temperature 2~4 hours, rate of cooling was 10 ℃/min~20 ℃/min.
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CN106466947B (en) * 2015-08-21 2019-10-25 华为技术有限公司 A kind of composite material and preparation method
CN106960706A (en) * 2017-04-07 2017-07-18 西安明科微电子材料有限公司 A kind of low temperature glass sintering process for sealing-in aluminium silicon carbide
CN109732077B (en) * 2019-01-23 2021-03-16 宁波合盛新材料有限公司 Fully-compact silicon carbide reinforced aluminum-based composite material billet and preparation method thereof
CN109576522B (en) * 2019-01-23 2020-01-14 宁波合盛新材料有限公司 Silicon carbide reinforced aluminum-based composite material and preparation method thereof
CN109676131B (en) * 2019-01-23 2021-02-19 宁波合盛新材料有限公司 Welding method of aluminum-based composite material
CN109702185B (en) * 2019-01-23 2021-04-06 宁波合盛新材料有限公司 Aluminum-based composite material forged piece and preparation method thereof
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CN115807184A (en) * 2022-09-07 2023-03-17 河南瀚银光电科技股份有限公司 High-performance silicon carbide particle reinforced aluminum matrix composite and preparation method thereof

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